CN103887361A - Precious-metal doped TiO2/TiO2 homogeneous-structure ultraviolet detector and preparation method - Google Patents
Precious-metal doped TiO2/TiO2 homogeneous-structure ultraviolet detector and preparation method Download PDFInfo
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- CN103887361A CN103887361A CN201410151399.3A CN201410151399A CN103887361A CN 103887361 A CN103887361 A CN 103887361A CN 201410151399 A CN201410151399 A CN 201410151399A CN 103887361 A CN103887361 A CN 103887361A
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- 239000010970 precious metal Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract 20
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 239000010453 quartz Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 71
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000004528 spin coating Methods 0.000 claims description 25
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 20
- 229920002120 photoresistant polymer Polymers 0.000 claims description 20
- 238000004544 sputter deposition Methods 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000003292 glue Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 239000010931 gold Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910000510 noble metal Inorganic materials 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000000295 complement effect Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000008236 heating water Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 claims description 2
- 229910001630 radium chloride Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 230000004044 response Effects 0.000 abstract description 12
- 230000005684 electric field Effects 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 8
- 230000004888 barrier function Effects 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 238000000825 ultraviolet detection Methods 0.000 description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier or surface barrier
- H01L31/103—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier or surface barrier the potential barrier being of the PN homojunction type
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0321—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 characterised by the doping material
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Abstract
The invention relates to a precious-metal doped TiO2/TiO2 homogeneous-structure ultraviolet detector and a preparation method and belongs to the technical field of semiconductor photoelectric devices. The detector comprises a quartz substrate, a precious-metal doped TiO2 film layer, a pure TiO2 film layer and a metal interdigital electrode. The detector is characterized by being provided with a homogeneous structure formed by the precious-metal doped TiO2 film layer and the pure TiO2 film layer. On one side, by the doping of precious metal, the substrate material has a low Fermi level, and the metal electrode and substrate material contacting barrier height is reduced; on the other side, the built-in electric field direction of the homogeneous structure formed by the precious-metal doped TiO2 film layer and the pure TiO2 film layer is opposite to the built-in electric field direction of metal-semiconductor contact of the detector, and the barrier height is also reduced. The photo-response characteristic of the ultraviolet detector is effectively improved from the material doping modification and the device structure.
Description
Technical field
The invention belongs to semiconductor photoelectric device technical field, be specifically related to a kind of TiO with precious metal doping
2/ TiO
2ultraviolet light detector of homostyructure and preparation method thereof.
Background technology
Ultraviolet detection technology is as the important branch of Modern Transducer Technology, be that a kind of laser that continues, infrared light and visible ray are surveyed another gate pole tool practicality in addition and the emerging Detection Techniques of using value, show potential prospect and using value in lightwave communication, imaging technique, environmental monitoring, combustion enginnering and following field such as energy storage and optoelectronic IC.
Along with the development of ultraviolet detection technology, the development of ultraviolet detector becomes the focus of concern.Military, civilian all in the urgent need to the ultraviolet detector of high reliability, high stability.The ultraviolet detector of pursuing high combination property seems particularly important.Researchers are devoted to improve by the whole bag of tricks the combination property of detector always in recent years, from basis material, the ultraviolet detector development that tradition homogenous material is matrix is comparatively ripe, novelty is little, and the exploration of some advanced composite material (ACM)s cannot obtain again high performance ultraviolet detector.Broad stopband oxide semiconductor has the characteristic of the brilliances such as energy gap is large, electron drift velocity is high, dielectric constant is little and potential technical advantage, shows huge development prospect in ultraviolet detection field.TiO
2owing to thering are excellent photoelectric properties, stable physicochemical characteristics and cheap price etc. receives much concern.But because the aspects such as material preparation, device architecture still exist defect, the photoelectric properties of ultraviolet detector are restricted, and device still awaits further raising in the parameter such as optical responsivity and response time.Therefore in order to prepare the TiO with higher response characteristics to light
2ultraviolet detector, by basis material TiO
2carry out doping vario-property or improve the methods such as device architecture and improve detector performance and become the hot issue of Recent study.
Noble metal is owing to having the work function higher than semiconductor and can introduce the features such as peculiar impurity energy level in forbidden band, can affect the transmission of semiconductor extinction characteristic, charge carrier and the barrier height of gold half contact etc., in semiconductor doping modification, have a extensive future.
Summary of the invention
The object of the present invention is to provide a kind of TiO with precious metal doping
2/ TiO
2ultraviolet light detector of homostyructure and preparation method thereof.The double-deck homostyructure that detector has has finally well improved the response characteristics to light of device.
Ultraviolet light detector of the present invention, is characterized in that: the TiO being adulterated by substrate (quartz substrate, Sapphire Substrate, silicon substrate etc.), noble metal (Pt, Au, Pd, Rh etc.) successively
2thin layer (molar concentration of precious metal doping is 0.008~0.04mol/L), pure TiO
2thin layer, metal interdigital electrode (metal is Au, Pt etc.) composition, the TiO of precious metal doping
2the thickness of thin layer is 150~210nm, pure TiO
2thin layer thickness is 30~90nm, and the thickness of metal interdigital electrode is 50~150nm, and electrode width is 5~60 μ m, and electrode spacing is 5~60 μ m.
The present invention adopts sol-gal process on substrate, to prepare successively the TiO of precious metal doping
2thin layer and pure TiO
2thin layer, then prepares metal interdigital electrode in the above.The device preparing like this has the TiO of precious metal doping
2thin layer and pure TiO
2the homostyructure that thin layer forms.On the one hand with pure TiO
2thin layer is compared, the TiO of precious metal doping
2thin layer is enough thick, and it,, as the main basis material of device, has lower Fermi level, is equivalent to TiO
2carry out acceptor doping, reduced the barrier height that metal electrode contacts with basis material; On the other hand, the thin layer of precious metal doping can be regarded as to one deck N-type lightly-doped layer (N-), it and TiO
2the internal electric field direction of the homostyructure (N--N) that layer forms and the internal electric field opposite direction that device itself gold half contacts, equally also reduced barrier height.The response characteristics to light of ultraviolet detector has effectively been improved in the final doping vario-property from material and device architecture two aspects.
A kind of TiO with precious metal doping of the present invention
2/ TiO
2ultraviolet light detector of homostyructure and preparation method thereof, its step is as follows:
[1] TiO
2the preparation of colloidal sol
Under room temperature, in the 5~10mL butyl titanate that 5~10mL acetic acid, 5~10mL acetylacetone,2,4-pentanedione, 5~10mL deionized water is splashed into continuous stirring successively and mix and the mixed liquor of 80~100mL ethanol, continue stirring until obtain the orange red colloidal sol of homogeneous transparent, ageing obtained TiO after 24~48 hours
2colloidal sol;
[2] precious metal doping TiO
2the preparation of colloidal sol
Get salt (chloroplatinic acid, the gold chloride of the noble metal of 0.1~0.3g, palladium bichloride, radium chloride etc.), added in the mixed liquor of 4mL~8mL water and 4~8mL ethanol, be stirred to abundant dissolving, the mixed liquor after dissolving added to the TiO of the 5~15mL taking out from step [1]
2in colloidal sol, 70~90 ℃ of heating water bath stirring 2~4h obtain the TiO of precious metal doping
2colloidal sol;
[3] cleaning of substrate
Substrate is put into acetone, ethanol and deionized water successively, and ultrasonic 10~15 minutes respectively, ultrasonic power was 80~100W, then flows down and dries up at nitrogen;
[4] precious metal doping TiO
2the preparation of film
The TiO of 5~7 layers of precious metal doping of spin coating on substrate after cleaning
2colloidal sol, the technique of every layer is: rotating speed 2000~3000rpm, even glue time 10~20s dries 5~7 minutes after even glue under 110~130 ℃ of conditions, then in air cooling 2~4 minutes; Finally by the substrate of good this colloidal sol of spin coating sintering 1.5~3 hours under 550~650 ℃ of conditions, thereby on substrate, form the TiO of precious metal doping
2film, thickness is 150~210nm;
[5] preparation of homostyructure
At the TiO of precious metal doping
21~3 layer of TiO of spin coating on thin layer
2colloidal sol, the technique of every layer is: rotating speed 2000~3000rpm, even glue time 10~20s dries 5~7 minutes after even glue under 110~130 ℃ of conditions, then in air cooling 2~4 minutes; Finally by good spin coating TiO
2the substrate of colloidal sol sintering 1.5~3 hours under 550~650 ℃ of conditions, thus the TiO by precious metal doping on substrate, obtained
2with pure TiO
2the homostyructure of bilayer film composition;
[6] preparation of metal interdigital electrode
At the thick BP212 eurymeric photoresist of first spin coating one deck 1~3 μ m in homostyructure surface preparing, be placed on hot plate under 70 ℃~90 ℃ conditions front baking 10~20 minutes; Then on mask aligner, to refer to that the mask plate of electrode pattern complementary structure and the photoresist layer of spin coating adjust close contact behind position with inserting, expose and develop 30~50 seconds after 50~60 seconds, with drying up after deionized water rinsing, then be placed on hot plate under 110 ℃~130 ℃ conditions post bake and after 15~25 minutes, on homostyructure layer, obtain needed photoresist and insert and refer to electrode pattern; Then adopt radiofrequency magnetron sputtering technology to prepare in the above electrode, sputtering chamber is evacuated to 2.0 × 10
-3~8.0 × 10
-3logical argon gas after Pa, sputtering pressure is 0.5~1.4Pa, and sputtering power is 60~110W, and sputtering time is 3~8 minutes; Finally with acetone by photoresist and metal is above ultrasonic etches away, ultrasonic power is 50~70W, the interdigital electrode thickness obtaining is 50~150nm, electrode width is 5~60 μ m, electrode spacing is 5~60 μ m; Finally prepare the TiO with precious metal doping by above step
2/ TiO
2the ultraviolet light detector of homostyructure.
Accompanying drawing explanation
Fig. 1: the structural representation of device of the present invention;
Fig. 2: TiO
2the X ray diffracting spectrum of film (embodiment 1);
Fig. 3: Pt/TiO
2the X ray diffracting spectrum of film (embodiment 2);
Fig. 4: under 300nm UV-irradiation, pure TiO
2ultraviolet detector (embodiment 1), Pt/TiO
2ultraviolet detector (embodiment 2) and there is the photoelectric current comparison diagram of the ultraviolet detector (embodiment 3) of homostyructure;
Fig. 5: pure TiO
2the response time figure of ultraviolet detector (embodiment 1);
Fig. 6: Pt/TiO
2the response time figure of ultraviolet detector (embodiment 2);
Fig. 7: the response time figure with the ultraviolet detector (embodiment 3) of homostyructure;
As shown in Figure 1, device is by substrate 1, Pt/TiO
2 thin layer 2, pure TiO
2 thin layer 3, metal interdigital electrode 4 form, and 300nm ultraviolet source 5 is radiated on photosensitive layer 2 and 3 and produces photo-generated carrier through substrate 1, under applying bias condition, are collected by metal interdigital electrode, produce photoelectric current, and photosensitive layer is by the Pt/TiO with homostyructure
2thin layer and TiO
2thin layer composition, the internal electric field opposite direction that its internal electric field direction contacts with semiconductor with metal electrode, makes potential barrier reduction, final optimization pass the response characteristics to light of device.
Fig. 2 is TiO
2the X ray diffracting spectrum of film, the position of all diffraction maximums and Detitanium-ore-type TiO
2(JCPDS No.21-1272) is corresponding for standard powder diffraction card, and the TiO of preparation is described
2there is the good crystalline structure of Detitanium-ore-type.
As shown in Figure 3, Pt/TiO
2in the X ray diffracting spectrum of film, occurred the diffraction maximum of Pt simple substance, illustrated that this part Pt is zeroth order, it enters into TiO in the mode of interstitial atom
2in lattice; In addition compared with standard powder diffraction card, TiO
2having there is slight shift left in the position of diffraction maximum own, illustrates that this part Pt has substituted TiO
2ti atom in lattice, is+4 valencys, according to bragg's formula: 2dsin θ=n λ, for certain n value, n λ is constant, and the diffraction angle of crystal interplanar distance d and X ray is inversely proportional to, and Pt atom enters TiO
2in lattice, by large its interplanar distance support, cause the angle of diffraction to diminish, there is skew in diffraction maximum position therefore.
As shown in Figure 4, curve 1,2,3 is respectively pure TiO
2ultraviolet detector, Pt/TiO
2ultraviolet detector and the ultraviolet detector with the homostyructure I-V curve chart under 300nm UV-irradiation; Under 5V bias voltage, photoelectric current is respectively 2.866 μ A, 35.711 μ A and 191.770 μ A.Pt/TiO
2the reason that ultraviolet detector photoelectric current increases is due at TiO
2in mix precious metals pt, basis material has lower Fermi level, has reduced the barrier height that metal electrode contacts with basis material; It is because Pt/TiO that the ultraviolet detector with homostyructure has maximum photoelectric current
2layer and TiO
2the internal electric field direction of the homostyructure (N--N) that layer forms and the internal electric field opposite direction that device itself gold half contacts, reduced barrier height to a greater degree.
Fig. 5 is pure TiO
2the response time curve of ultraviolet detector, as shown in the figure, the rise time is 2.284s, be 1.721s fall time.
Fig. 6 is Pt/TiO
2ultraviolet detector response time curve, as shown in the figure, the rise time foreshortens to 1.517s, and be 1.672s fall time.
Fig. 7 is the ultraviolet detector response time curve with homostyructure, and as shown in the figure, the rise time is only 861.6ms, and be 1.788s fall time.
Embodiment
Embodiment 1:
[1] under room temperature, in the 8mL butyl titanate that 8mL acetic acid, 8mL acetylacetone,2,4-pentanedione, 8mL deionized water is splashed into continuous stirring successively and mix and the mixed liquor of 90mL ethanol, continue stirring until obtain the orange red colloidal sol of homogeneous transparent, ageing obtained TiO after 36 hours
2colloidal sol;
[2] quartz substrate is put into acetone, ethanol and deionized water successively, ultrasonic 12 minutes respectively, ultrasonic power was 90W, then flows down and dries up at nitrogen;
[3] in the quartz substrate after cleaning, use 6 layers of TiO of sol evenning machine spin coating
2colloidal sol, the rotating speed of every layer is 2500rpm, and the even glue time is 15s, dries 6 minutes in air cooling 3 minutes after even glue under 120 ℃ of conditions; Finally by good spin coating TiO
2the substrate slice of colloidal sol is placed in Muffle furnace, and under 600 ℃ of conditions, sintering 2 hours, forms Detitanium-ore-type TiO
2film, thickness is about 180nm;
[4] TiO preparing
2the thick BP212 eurymeric photoresist of the first spin coating one deck 1.5 μ m of film surface, is placed on hot plate under 80 ℃ of conditions front baking 15 minutes; Then on mask aligner, to refer to that the mask plate of electrode pattern complementary structure and the photoresist layer of spin coating adjust close contact behind position with inserting, expose and develop 40 seconds after 55 seconds, with drying up after deionized water rinsing, be placed on hot plate under 120 ℃ of conditions post bake and after 20 minutes, on film, obtain needed photoresist and insert and refer to electrode pattern; Then adopt radiofrequency magnetron sputtering technology to prepare in the above Au electrode, sputtering chamber is evacuated to 3.0 × 10
-3logical argon gas after Pa, sputtering pressure is 1.2Pa, and sputtering power is 100W, and sputtering time is 6 minutes; Finally with acetone by photoresist and metal is above ultrasonic etches away, ultrasonic power is 60W, the interdigital electrode thickness obtaining is 120nm, electrode width is 20 μ m, electrode spacing is 20 μ m; Prepare pure TiO by above step
2ultraviolet light detector.Photoelectric current under 5V bias voltage 300nm UV-irradiation is 2.866 μ A; Rise time is 2.284s, and be 1.721s fall time.
Embodiment 2:
[1] under room temperature, in the 8mL butyl titanate that 8mL acetic acid, 8mL acetylacetone,2,4-pentanedione, 8mL deionized water is splashed into continuous stirring successively and mix and the mixed liquor of 90mL ethanol, continue stirring until obtain the orange red colloidal sol of homogeneous transparent, ageing obtained TiO after 36 hours
2colloidal sol;
[2] get the chloroplatinic acid (H of 0.2g
2ptCl
66H
2o), added in the mixed liquor of 5mL water and 5mL ethanol, be stirred to abundant dissolving, the mixed liquor after dissolving is added to the TiO of the 10mL taking out from step [1]
2in colloidal sol, 80 ℃ of heating water baths stir 3h and obtain Pt/TiO
2colloidal sol;
[3] quartz substrate is put into acetone, ethanol and deionized water successively, ultrasonic 12 minutes respectively, ultrasonic power was 90W, then flows down and dries up at nitrogen;
[4] in the quartz substrate after cleaning, use 6 layers of Pt/TiO of sol evenning machine spin coating
2colloidal sol, the rotating speed of every layer is 2500rpm, and the even glue time is 15s, dries 6 minutes in air cooling 3 minutes after even glue under 120 ℃ of conditions; Finally by good spin coating Pt/TiO
2the substrate slice of colloidal sol is placed in Muffle furnace, and under 600 ℃ of conditions, sintering 2 hours, forms Pt/TiO
2film, thickness is about 180nm;
[5] Pt/TiO preparing
2the thick BP212 eurymeric photoresist of the first spin coating one deck 1.5 μ m of film surface, is placed on hot plate under 80 ℃ of conditions front baking 15 minutes; Then on mask aligner, to refer to that the mask plate of electrode pattern complementary structure and the photoresist layer of spin coating adjust close contact behind position with inserting, expose and develop 40 seconds after 55 seconds, with drying up after deionized water rinsing, be placed on hot plate under 120 ℃ of conditions post bake and after 20 minutes, on film, obtain needed photoresist and insert and refer to electrode pattern; Then adopt radiofrequency magnetron sputtering technology to prepare in the above Au electrode, sputtering chamber is evacuated to 3.0 × 10
-3logical argon gas after Pa, sputtering pressure is 1.2Pa, and sputtering power is 100W, and sputtering time is 6 minutes; Finally with acetone by photoresist and metal is above ultrasonic etches away, ultrasonic power is 60W, the interdigital electrode thickness obtaining is 120nm, electrode width is 20 μ m, electrode spacing is 20 μ m; Prepare Pt/TiO by above step
2ultraviolet light detector.With pure TiO
2ultraviolet detector is compared photoelectric current and has been improved 12.5 times, and the rise time has shortened 1.5 times.
Embodiment 3:
[1] under room temperature, in the 8mL butyl titanate that 8mL acetic acid, 8mL acetylacetone,2,4-pentanedione, 8mL deionized water is splashed into continuous stirring successively and mix and the mixed liquor of 90mL ethanol, continue stirring until obtain the orange red colloidal sol of homogeneous transparent, ageing obtained TiO after 36 hours
2colloidal sol;
[2] get the chloroplatinic acid (H of 0.2g
2ptCl
66H
2o), added in the mixed liquor of 5mL water and 5mL ethanol, be stirred to abundant dissolving, the mixed liquor after dissolving is added to the TiO of the 10mL taking out from step [1]
2in colloidal sol, 80 ℃ of heating water baths stir 3h and obtain Pt/TiO
2colloidal sol;
[3] quartz substrate is put into acetone, ethanol and deionized water successively, ultrasonic 12 minutes respectively, ultrasonic power was 90W, then flows down and dries up at nitrogen;
[4] in the quartz substrate after cleaning, use 5 layers of Pt/TiO of sol evenning machine spin coating
2colloidal sol, the rotating speed of every layer is 2500rpm, and the even glue time is 15s, dries 6 minutes in air cooling 3 minutes after even glue under 120 ℃ of conditions; Finally by good spin coating Pt/TiO
2the substrate slice of colloidal sol is placed in Muffle furnace, and under 600 ℃ of conditions, sintering 2 hours, forms Pt/TiO
2film, thickness is about 150nm;
[5] at Pt/TiO
2on thin layer, again prepare pure TiO
2thin layer (1 layer of TiO of spin coating
2colloidal sol, rotating speed is 2500rpm, the even glue time is 15s, dries 6 minutes in air cooling 3 minutes under 120 ℃ of conditions; Under 600 ℃ of conditions in Muffle furnace sintering 2 hours, the TiO preparing
2film thickness is about 30nm), on substrate, form by Pt/TiO like this
2with pure TiO
2the homostyructure of bilayer film composition, thickness is about 180nm;
[6], at the thick BP212 eurymeric photoresist of the first spin coating one deck 1.5 μ m in homostyructure surface preparing, be placed on hot plate under 80 ℃ of conditions front baking 15 minutes; Then on mask aligner, to refer to that the mask plate of electrode pattern complementary structure and the photoresist layer of spin coating adjust close contact behind position with inserting, expose and develop 40 seconds after 55 seconds, with drying up after deionized water rinsing, be placed on hot plate under 120 ℃ of conditions post bake and after 20 minutes, on film, obtain needed photoresist and insert and refer to electrode pattern; Then adopt radiofrequency magnetron sputtering technology to prepare in the above Au electrode, sputtering chamber is evacuated to 3.0 × 10
-3logical argon gas after Pa, sputtering pressure is 1.2Pa, and sputtering power is 100W, and sputtering time is 6 minutes; Finally with acetone by photoresist and metal is above ultrasonic etches away, ultrasonic power is 60W, the interdigital electrode thickness obtaining is 120nm, electrode width is 20 μ m, electrode spacing is 20 μ m; Prepare the TiO with precious metal doping by above step
2/ TiO
2the ultraviolet light detector of homostyructure.With pure TiO
2ultraviolet detector is compared photoelectric current and has been improved approximately 67 times, and the rise time has shortened 2.65 times.
In above-described embodiment, I-V curve is to measure with Keithley2601.All tests are all carried out under atmospheric environment.
Above said content, is only the specific embodiment of the present invention, can not limit scope of the invention process with it, and the impartial changes and improvements of generally carrying out according to patent claim of the present invention, all should still belong to the scope that patent of the present invention contains.
Claims (9)
1. one kind has the TiO of precious metal doping
2/ TiO
2the ultraviolet detector of homostyructure, is characterized in that: successively by the TiO of substrate, precious metal doping
2thin layer, pure TiO
2thin layer, metal interdigital electrode composition, wherein, the TiO of precious metal doping
2in thin layer, the molar concentration of precious metal doping is 0.008~0.04mol/L.
2. a kind of TiO with precious metal doping as claimed in claim 1
2/ TiO
2the ultraviolet detector of homostyructure, is characterized in that: the TiO of precious metal doping
2the thickness of thin layer is 150~210nm, pure TiO
2the thickness of thin layer is 30~90nm, and the thickness of metal interdigital electrode is 50~150nm, and electrode width is 5~60 μ m, and electrode spacing is 5~60 μ m.
3. a kind of TiO with precious metal doping as claimed in claim 1 or 2
2/ TiO
2the ultraviolet detector of homostyructure, is characterized in that: substrate is quartz, sapphire or silicon, and noble metal is Pt, Au, Pd or Rh, and metal interdigital electrode is Au or Pt.
4. one kind has the TiO of precious metal doping
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, its step is as follows:
[1] precious metal doping TiO
2the preparation of film
The TiO of 5~7 layers of precious metal doping of spin coating on substrate after cleaning
2colloidal sol, the technique of every layer is: rotating speed 2000~3000rpm, even glue time 10~20s dries 5~7 minutes after even glue under 110~130 ℃ of conditions, then in air cooling 2~4 minutes; Finally by the substrate of good this colloidal sol of spin coating sintering 1.5~3 hours under 550~650 ℃ of conditions, thereby on substrate, form the TiO of precious metal doping
2film, thickness is 150~210nm;
[2] preparation of homostyructure
At the TiO of precious metal doping
21~3 layer of TiO of spin coating on film
2colloidal sol, the technique of every layer is: rotating speed 2000~3000rpm, even glue time 10~20s dries 5~7 minutes after even glue under 110~130 ℃ of conditions, then in air cooling 2~4 minutes; Finally by good spin coating TiO
2the substrate of colloidal sol sintering 1.5~3 hours under 550~650 ℃ of conditions, thus the TiO by precious metal doping on substrate, obtained
2with pure TiO
2the homostyructure of bilayer film composition;
[3] preparation of metal interdigital electrode
In the homostyructure surface metal interdigital electrode preparing, thickness of electrode is 50~150nm, and electrode width is 5~60 μ m, and electrode spacing is 5~60 μ m; Finally prepare the TiO with precious metal doping by above step
2/ TiO
2the ultraviolet light detector of homostyructure.
5. the TiO with precious metal doping as claimed in claim 4
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, is characterized in that: TiO
2the preparation of colloidal sol, under room temperature, in the 5~10mL butyl titanate that 5~10mL acetic acid, 5~10mL acetylacetone,2,4-pentanedione, 5~10mL deionized water is splashed into continuous stirring successively and mix and the mixed liquor of 80~100mL ethanol, continue stirring until obtain the orange red colloidal sol of homogeneous transparent, ageing obtained TiO after 24~48 hours
2colloidal sol.
6. the TiO with precious metal doping as claimed in claim 4
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, is characterized in that: precious metal doping TiO
2the preparation of colloidal sol, is the salt of getting the noble metal of 0.1~0.3g, is added in the mixed liquor of 4mL~8mL water and 4~8mL ethanol, is stirred to abundant dissolving, the mixed liquor after dissolving is added to the TiO of the 5~15mL taking out from step [1]
2in colloidal sol, 70~90 ℃ of heating water bath stirring 2~4h obtain the TiO of precious metal doping
2colloidal sol.
7. the TiO with precious metal doping as claimed in claim 6
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, is characterized in that: the salt of noble metal is chloroplatinic acid, gold chloride, palladium bichloride or radium chloride.
8. the TiO with precious metal doping as claimed in claim 4
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, it is characterized in that: insert the preparation that refers to electrode, be at the thick BP212 eurymeric photoresist of first spin coating one deck 1~3 μ m in homostyructure surface preparing, be placed on hot plate under 70 ℃~90 ℃ conditions front baking 10~20 minutes; Then on mask aligner, to refer to that the mask plate of electrode pattern complementary structure and the photoresist layer of spin coating adjust close contact behind position with inserting, expose and develop 30~50 seconds after 50~60 seconds, with drying up after deionized water rinsing, then be placed on hot plate under 110 ℃~130 ℃ conditions post bake and after 15~25 minutes, on homostyructure layer, obtain needed photoresist and insert and refer to electrode pattern; Then adopt radiofrequency magnetron sputtering technology to prepare in the above electrode, sputtering chamber is evacuated to 2.0 × 10
-3~8.0 × 10
-3logical argon gas after Pa, sputtering pressure is 0.5~1.4Pa, and sputtering power is 60~110W, and sputtering time is 3~8 minutes; Finally with acetone by photoresist and metal is above ultrasonic etches away, ultrasonic power is 50~70W, thereby obtains metal interdigital electrode.
9. the TiO with precious metal doping as claimed in claim 4
2/ TiO
2the preparation method of the ultraviolet detector of homostyructure, is characterized in that: metal interdigital electrode is Au or Pt.
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